CN114836621B - Process and device for extracting lithium by using carbonic acid type salt lake adsorption method - Google Patents
Process and device for extracting lithium by using carbonic acid type salt lake adsorption method Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 47
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 36
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 title description 2
- 239000003463 adsorbent Substances 0.000 claims abstract description 34
- 239000012267 brine Substances 0.000 claims abstract description 34
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 34
- VVNXEADCOVSAER-UHFFFAOYSA-N lithium sodium Chemical compound [Li].[Na] VVNXEADCOVSAER-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000012452 mother liquor Substances 0.000 claims abstract description 31
- 238000003795 desorption Methods 0.000 claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 22
- 239000012528 membrane Substances 0.000 claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 14
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 24
- 239000003513 alkali Substances 0.000 claims description 23
- 238000002425 crystallisation Methods 0.000 claims description 17
- 230000008025 crystallization Effects 0.000 claims description 17
- 150000005323 carbonate salts Chemical class 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 8
- SWAIALBIBWIKKQ-UHFFFAOYSA-N lithium titanium Chemical compound [Li].[Ti] SWAIALBIBWIKKQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 16
- 229910052719 titanium Inorganic materials 0.000 description 16
- 239000010936 titanium Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 239000012670 alkaline solution Substances 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 239000003480 eluent Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 3
- 239000010413 mother solution Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/14—Alkali metal compounds
- C25B1/16—Hydroxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Mechanical Engineering (AREA)
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Abstract
The invention relates to a process for extracting lithium by a carbonate type salt lake adsorption method, and belongs to the technical field of lithium extraction of salt lakes. In the process of extracting lithium from brine by an adsorption method, the adsorption process is divided into two stages, wherein the first stage adopts an adsorbent to adsorb the brine, and the second stage adopts the adsorbent to adsorb bipolar membrane alkaline liquor concentrated mother liquor in a subsequent working section, so that lithium ions in the mother liquor replace sodium ions on the adsorbent, the finally obtained desorption solution has lower sodium-lithium ratio, and the purity of the extracted lithium is improved.
Description
Technical Field
The invention relates to a process for extracting lithium from carbonate type salt lake brine by an adsorption method, and belongs to the technical field of lithium extraction from salt lakes.
Background
In recent years, with the rapid development of industries such as nuclear power, aerospace, lithium electric automobiles and the like, the global demand for lithium products is increasing year by year. The report of the united states geological exploration bureau in 2017 shows that salt lake brine lithium resources account for about 58% of world lithium resources, and salt lake lithium extraction becomes a trend of global future lithium mine development. In the prior art, when extracting lithium from a carbonate salt lake, a titanium adsorbent may be used to perform the steps of adsorption, desorption, separation and purification of lithium ions. The method has the advantages of simple process, no environmental pollution and the like, and is more suitable for recovering lithium from brine with high sodium-lithium ratio compared with other methods.
However, for some carbonate salt lake brine, the sodium ion concentration is far higher than the lithium ion concentration, the sodium-lithium mass ratio is higher than 100, and the quality of sodium and lithium in qualified liquid obtained after adsorption-desorption by the titanium-based adsorbent is higher (more than or equal to 2.5), which is unfavorable for subsequent separation, purification and concentration working sections and affects the purity of the final lithium product.
Patent CN106241839 a discloses a method for separating magnesium and reducing magnesium-lithium ratio from salt lake old brine, which comprises the following steps of old brine, membrane distillation concentration and crystallization separation; the beneficial effects of the invention are as follows: the molar ratio of magnesium and lithium in the old brine of the salt lake is reduced to be less than 1, and the magnesium and lithium is used as a raw material liquid which is conventional and is suitable for a magnesium and lithium separation method in the salt lake brine with a medium-low magnesium and lithium ratio, such as a solvent extraction method, an ion exchange adsorption method and the like, so that the thorough separation of magnesium and lithium is realized, and the key technology of the salt lake development is realized. The patent only aims at the old brine of the salt lake with high magnesium-lithium ratio, solves the problem of magnesium-lithium separation, and is not applicable to the salt lake brine with high sodium-lithium ratio.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: in the process of absorbing and extracting lithium from carbonate brine by adopting a titanium adsorbent, the sodium-lithium ratio in the desorption liquid is high due to the fact that sodium-lithium ratio in the brine is high, and the purity of extracted lithium is influenced. The invention has the following points: in the process of extracting lithium from brine by an adsorption method, the adsorption process is divided into two stages, wherein the first stage adopts an adsorbent to adsorb the brine, and the second stage adopts the adsorbent to adsorb bipolar membrane alkaline liquor concentrated mother liquor of a subsequent working section, so that lithium ions in the mother liquor replace sodium ions on the adsorbent, the finally obtained desorption solution has a lower sodium-lithium ratio, and the purity of the extracted lithium is improved.
The technical proposal is as follows:
the lithium extracting process with carbonate salt lake adsorption process includes the following steps:
step 1, absorbing carbonate salt lake brine by adopting a titanium lithium ion sieve adsorbent;
step 2, continuing to adopt the adsorbent obtained in the step 1 to adsorb mother liquor produced after the bipolar membrane alkali liquor is crystallized;
step 3, desorbing the adsorbent obtained in the step 2;
step 4, carrying out bipolar membrane electrolysis treatment on the desorption solution to obtain acid liquor and alkali liquor;
step 5, concentrating alkali liquor, and crystallizing to obtain LiOH; and obtaining mother liquor produced after bipolar membrane alkali liquor crystallization.
The alkaline solution with high sodium-lithium ratio in the step 1 can be one or two mixed solutions of carbonate salt lake brine and lithium precipitation mother liquor.
And in the step 1, the sodium-lithium ratio of the carbonate salt lake brine is more than 45.
And 2, the sodium-lithium ratio of the mother solution produced after the bipolar membrane alkali liquor is crystallized in the step 2 is 2-8, wherein the lithium concentration is 10-25 g/L.
And 3. The sodium-lithium ratio of the desorption solution obtained by the desorption treatment in the step 3 is less than 1.5.
The utility model provides a carbonate formula salt lake adsorption process draws lithium device, includes:
the adsorption device is filled with a titanium lithium ion sieve adsorbent and is used for adsorbing lithium in brine;
the bipolar membrane is connected with the adsorption device and is used for carrying out bipolar membrane electrolysis treatment on desorption liquid of the adsorption device;
the concentration device is connected to the alkali liquor outlet of the bipolar membrane and is used for concentrating alkali liquor;
the solid-liquid separator is connected with the concentration device and is used for separating out LiOH separated out after concentration;
the alkali liquor outlet of the bipolar membrane is connected with the feed liquor inlet on the adsorption device.
In one embodiment, an acid outlet is further arranged on the bipolar membrane.
In one embodiment, the adsorption device is further provided with a desorption liquid inlet.
In one embodiment, the concentrating device is an evaporative concentrator.
In one embodiment, the solid-liquid separator is a centrifuge.
In one embodiment, the brine adding port is connected with the feed liquid inlet.
Advantageous effects
(1) Directly making the titanium-based adsorbent adsorb alkaline solution with high sodium-lithium ratio, and desorbing to obtain qualified solution with high sodium-lithium ratio (more than or equal to 2.5), wherein the titanium-based adsorbent can adsorb part of sodium ions in the alkaline solution with high sodium-lithium ratio; firstly, the titanium-based adsorbent adsorbs an alkaline solution with a high sodium-lithium ratio, then adsorbs an alkaline solution with a low sodium-lithium ratio, and the lithium ions in the alkaline solution with the low sodium-lithium ratio can be replaced with part of sodium ions in the titanium-based adsorbent, so that the sodium-lithium ratio in the qualified liquid obtained by desorption is low (less than or equal to 1.5), and the purpose of reducing the sodium-lithium ratio of the qualified liquid is achieved.
(2) The crystallization mother liquor obtained by evaporating and concentrating alkali liquor generated by the bipolar membrane is just alkaline solution with low sodium-lithium ratio, and the lithium concentration is higher, so that compared with carbonate type salt lake brine or lithium precipitation mother liquor, the driving force of the titanium adsorbent for adsorbing lithium in the crystallization mother liquor is larger, therefore, after the titanium adsorbent adsorbs carbonate type salt lake brine or lithium precipitation mother liquor, the titanium adsorbent can still continuously adsorb the crystallization mother liquor, and the lithium in the crystallization mother liquor is recovered, so that the aim of improving the overall lithium yield is fulfilled.
Drawings
FIG. 1 is a diagram of an apparatus of the present invention;
wherein, 1, an adsorption device; 2. a bipolar membrane; 3. a concentrating device; 4. a solid-liquid separator; 5. an acid liquor outlet; 6. an alkali liquor outlet; 7. a feed liquid inlet; 8. a brine inlet; 9. a desorption liquid inlet;
Detailed Description
The basic properties of brine in the invention are as follows: na (Na) + =140 g/L，Li + =0.9 g/L，K + =35 g/L，Mg 2+ =0.02 g/L ，CO 3 2- =30 g/L，Cl - =150 g/L，pH=10。
The invention solves the problem of separating sodium and lithium in salt lake brine with high sodium-lithium ratio, adopts a mode of sequential adsorption by stages, and adopts a titanium adsorbent to adsorb carbonate salt lake brine (the sodium-lithium ratio, the lithium concentration is lower than 1.2 g/L) in the first stage; and in the second stage, the lithium ions in the crystallization mother liquor of the second stage are utilized to replace the sodium ions adsorbed by the titanium adsorbent in the first stage, so that the purpose of reducing the sodium-lithium ratio of the qualified liquor is realized, and the total yield of lithium is improved.
Example 1
And (3) adsorbing carbonate brine by using a titanium lithium ion sieve adsorbent. The adsorption process temperature is 25 ℃ and the flow rate is 20BV/h. The adsorption time is 1h, after the adsorption is completed, the subsequent crystallization mother liquor is adopted for adsorption, the temperature during the re-adsorption is 25 ℃, the flow rate is 2BV/h, and the adsorption saturation time is 0.5h.
And eluting the titanium adsorbent to obtain desorption liquid, wherein 0.2mol/L dilute hydrochloric acid is used as eluent in the eluting process, the flow rate is 10BV/h, the temperature is 25 ℃, and the desorption time is 0.5h. The sodium-lithium ratio of the desorption liquid is 1.
The crystallization mother liquor is derived from the following steps:
after the desorption solution is electrolyzed by adopting a bipolar membrane, an acid solution (HCl, the H+ concentration is about 2.36 mol/L) and an alkali solution (NaOH and LiOH, the concentrations are 0.55mol/L and 1.84mol/L respectively) are obtained, the alkali solution is concentrated and crystallized to obtain LiOH (final target product, the purity of the product is 99.9 percent and the Na content is 0.1 percent), mother solution is obtained in the crystallization process, and the main ion components in the mother solution are K+, na+ and Li+.
Example 2
And (3) adsorbing carbonate brine by using a titanium lithium ion sieve adsorbent. The adsorption process temperature is 20 ℃ and the flow rate is 15BV/h. The adsorption time is 1.5h, after the adsorption is completed, the subsequent crystallization mother liquor is adopted for adsorption, the temperature during the re-adsorption is 20 ℃, the flow rate is 1.5BV/h, and the adsorption saturation time is 1h.
And eluting the titanium adsorbent to obtain desorption liquid, wherein 0.25mol/L dilute hydrochloric acid is used as eluent in the eluting process, the flow rate is 12BV/h, the temperature is 20 ℃, and the desorption time is 1h. The sodium-lithium ratio of the desorption liquid is 1.2.
The crystallization mother liquor is derived from the following steps:
electrolysis of desorption solution by bipolar membraneThereafter, an acid solution (HCl, H) was obtained + Concentration of about 2.42 mol/L) and alkali solution (NaOH and LiOH, concentration of 0.59mol/L and 1.80mol/L respectively), concentrating and crystallizing the alkali solution to obtain LiOH (final target product, product purity of 99.9% and Na content of 0.11%), and crystallizing to obtain mother liquor, wherein the main ion component in the mother liquor is K + 、Na + And Li (lithium) + 。
Example 3
And (3) adsorbing carbonate brine by using a titanium lithium ion sieve adsorbent. The adsorption process temperature is 30 ℃ and the flow rate is 22BV/h. The adsorption time is 0.5h, after the adsorption is completed, the subsequent crystallization mother liquor is adopted for adsorption, the temperature during the re-adsorption is 30 ℃, the flow rate is 1.5BV/h, and the adsorption saturation time is 0.5h.
And eluting the titanium adsorbent to obtain desorption liquid, wherein 0.1mol/L dilute hydrochloric acid is used as eluent in the eluting process, the flow rate is 8BV/h, the temperature is 30 ℃, and the desorption time is 1h. The sodium-lithium ratio of the desorption liquid is 0.9.
The crystallization mother liquor is derived from the following steps:
the desorption solution is electrolyzed by a bipolar membrane to obtain acid liquor (HCl, H) + Concentration of about 2.21 mol/L) and alkali solution (NaOH and LiOH, concentration of 0.51mol/L and 1.93mol/L respectively), concentrating and crystallizing the alkali solution to obtain LiOH (final target product, product purity of 99.9%, na content of 0.08%), and crystallizing to obtain mother liquor, wherein the main ion component in the mother liquor is K + 、Na + And Li (lithium) + 。
Comparative example 1
The difference from example 1 is that: the secondary adsorption treatment is not carried out on the adsorbent by adopting the crystallization mother liquor.
And (3) adsorbing carbonate brine by using a titanium lithium ion sieve adsorbent. The adsorption process temperature is 25 ℃ and the flow rate is 20BV/h. The adsorption time was 1h.
And eluting the titanium adsorbent after adsorption to obtain desorption liquid, wherein 0.2mol/L dilute hydrochloric acid is used as eluent, the flow rate is 10BV/h, the temperature is 25 ℃, and the desorption time is 0.5h. The sodium-lithium ratio of the desorption solution was 2.5.
Desorbing liquidAfter electrolysis using bipolar membranes, acid solutions (HCl, H) are obtained + Concentration of about 2.67 mol/L) and alkali solution (NaOH and LiOH, concentration of 0.71mol/L and 1.81mol/L respectively), concentrating and crystallizing the alkali solution to obtain LiOH (final target product, product purity of 99.1%, na content of 0.5%), and crystallizing to obtain mother liquor, wherein the main ion component in the mother liquor is K + 、Na + And Li (lithium) + 。
By comparing the embodiment 1 with the comparative embodiment 1, after the crystallization mother liquor is used for reconversion, the sodium-lithium ratio in the desorption liquid is effectively reduced, so that the content of the finally obtained LiOH component is improved; in addition, the waste materials in the production process are effectively utilized, so that the resource utilization rate is higher.
Claims (2)
1. The process for extracting lithium by using carbonate salt lake brine adsorption method is characterized by comprising the following steps of:
step 1, absorbing carbonate salt lake brine by adopting a titanium lithium ion sieve adsorbent; the sodium-lithium ratio of carbonate salt lake brine is more than 45;
step 2, continuing to adopt the adsorbent obtained in the step 1 to adsorb mother liquor produced after the bipolar membrane alkali liquor is crystallized; the sodium-lithium ratio range of the mother liquor produced after the bipolar membrane alkali liquor is crystallized is 2-8, wherein the lithium concentration is 10-25 g/L;
step 3, desorbing the adsorbent obtained in the step 2;
step 4, carrying out bipolar membrane electrolysis treatment on the desorption solution to obtain acid liquor and alkali liquor;
step 5, concentrating and crystallizing the alkali liquor to obtain LiOH; and obtaining mother liquor produced after bipolar membrane alkali liquor crystallization.
2. The process for extracting lithium by using a carbonate salt lake adsorption method according to claim 1, wherein the sodium-lithium ratio of the desorption solution obtained by the desorption treatment in the 3 rd step is less than 1.5.
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